Case Ditails

Case Name Explosion due to temperature rise from careless handling in the nitrosation reaction
Pictograph
Date November 5, 1962
Place Ube, Yamaguchi, Japan
Location Laboratory
Overview In the experiment on the nitrosation of benzoic acid, an explosion occurred because the temperature was raised too high for the improvement in the yield, and two persons got injured. Thermal hazard of the used reagent was confirmed in the study of safety beforehand. However, an injury accident happened because thermal instability of the mixture had not understood and enough protection in case of emergency has not been prepared.
Incident An explosion occurred under experiment on the nitrosation of benzoic acid in the laboratory of the factory, and two persons got injured.
Processing Research and development
Process Flow Fig3.Unit process flow
Chemical Reaction Nitrosation
Chemical Equation Fig2.Chemical reaction formula
Substance Benzoic acid, Fig4
Nitrosyl perchlorate, Fig5
Perchloric acid, Fig6
Type of Accident Explosion
Sequence 4.1g of benzoic acid, 3.8g of perchloric nitrosyl, and 15g of 70% perchloric acid aqueous solution were mixed. An explosion occurred while temperature rose up to 98-99 °C with stirring.
Cause An explosion occurred because the temperature was raised too high for improving the yield. A sufficient yield was not obtained when it was raised up to 90 °C in the last experiment, so the next experiment was conducted at higher temperature to raise the yield. It had been confirmed that the reagent used for the experiment was comparatively stable below 100 °C, in case existing separately. However, it was not confirmed beforehand that the mixture decomposed exothermally at about 100 °C and generated carbon dioxide.
Countermeasures 1. Safety education and training are carried out to the experiment staff beforehand.
2. The facilities which protect the experiment staff are prepared.
Knowledge Comment 1. As unknown matters are tried in the experiment, previous safety study on operation is necessary.
2. Unexpected reactions sometimes occur especially in the experiment on the chemical reaction. Therefore, the facilities that protect the experiment staff must be prepared.
3. Even stable chemicals in case existing separately, it might become unstable if it is mixed with other materials.
Background 1. Insufficient study of hazard factors before the experiment.
2. There were the defects of protection facilities for the experiment staff.
Reason for Adding to DB Example of accident caused dueto insufficient investigationon safety of the experiment
Scenario
Primary Scenario Insufficient Analysis or Research, Insufficient Prior Research, No Check of Thermal Stability, Carelessness, Insufficient Understanding, Insufficient Recognition of Risk, Poor Value Perception, Poor Safety Awareness, Insuficient Education/Training for Safety, Nitrosation Reaction, Malicious Act, Rule Violation, Safety Rule Violation, Non-Regular Action, Change, Temperature Rise, Bad Event, Chemical Phenomenon, Unexpected Reaction, Secondary Damage, External Damage, Explosion, Bodily Harm, Injury, 2 person injured
Sources Masamitsu Tamura, Masahide Wakakura, Explosion under nitrosation reaction, Reaction danger -Accident case and analysis -, p.86(1995).
Number of Injuries 2
Financial Cost ¥ 2,550
Multimedia Files Fig4.Chemical formula
Fig5.Chemical formula
Fig6.Chemical formula
Field Chemicals and Plants
Author OGAWA, Terushige (Graduate School of Environment and Information Sciences, Yokohama National University)
TAMURA, Masamitsu (Center for Risk Management and Safety Sciences, Yokohama National University)